CN105424673B - The SERS substrates and preparation method of carried noble metal nano-cluster with 3D reticulated structures - Google Patents
The SERS substrates and preparation method of carried noble metal nano-cluster with 3D reticulated structures Download PDFInfo
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- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
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Abstract
The present invention provides a kind of new SERS substrates of carried noble metal nano-cluster with 3D reticulated structures and preparation method thereof, the carbon fiber for being loaded with cobalt acid nanosized nickel rods is prepared using hydro-thermal reaction method, make periodicity 3D network structure of the cobalt acid nanosized nickel rods in grown on carbon fibers for rule, then noble metal nano particles are coated on the above-mentioned carbon fiber surface for being loaded with cobalt acid nanosized nickel rods using magnetron sputtering technique, obtain the SERS substrates of the carried noble metal nano-cluster with 3D reticulated structures.It is characterized in that the netted stereochemical structure cobalt acid nickel of the 3D to be formed has abundant tip and even curface, is advantageous to noble metal nano particles and forms substantial amounts of cluster structure thereon, produce stronger SERS signal.Meanwhile periodic structure causes SERS focuses to be uniformly distributed, there is the signal output of stable uniform in actually detected.Further, since carrier is carbon fiber, makes the SERS substrates of preparation flexible, can cut, it is portable, it is easy to be applied to clinical biochemical medicine detection.
Description
Technical field
The present invention relates to material engineering and field of nanometer technology, specifically, is related to a kind of negative with 3D reticulated structures
The SERS substrates and preparation method of supported noble metal nano-cluster.
Background technology
In recent years, because noble metal nano particles have excellent catalysis, electrical and optical properties, it has been widely used
In fields such as chemical reaction, drug delivery, microelectronics and bio-sensings.In bio-sensing field, noble metal nano particles are usual
SERS (SERS) substrate is used as, SERS technologies have excellent dactylogram evident characteristics, thus energy
Enough test substance of the detection with extremely low concentration.This sensitive detectivity is mainly based upon the local of noble metal nano particles
Surface plasma body resonant vibration characteristic forms the local electromagnetic field of enhancing.So far, to further enhance SERS signal intensity,
A large amount of noble metal nano particles with unique morphology are developed, such as nanometer dimer, nanocube and is received nanometer star
Rice sea urchin etc. obtains higher local electromagnetic field intensity.But because noble metal has higher chemism, it is general these
Nano material with special appearance is easily deformed, and then loses SERS activity.And the preparation technology of these structures is complicated, into
This is higher, and the residue of surfactant and reducing agent for being used in experiment etc. easily pollutes environment.Therefore, although with relative
Relatively low SERS activity, but have the advantages that preparation method is simple and the stable spherical noble metal nano particles of property still by
It is widely used.Therefore, how present study hotspot obtains the cluster structure of noble metal nano ball to further enhance it if turning to
SERS signal.
The content of the invention
It is an object of the invention to provide a kind of SERS bases of the new carried noble metal nano-cluster with 3D reticulated structures
Bottom and preparation method thereof.
In order to realize the object of the invention, the SERS of the carried noble metal nano-cluster provided by the invention with 3D reticulated structures
The preparation method of substrate, it is that the carbon fiber that cobalt acid nanosized nickel rods are loaded with using the preparation of hydro-thermal reaction method (is loaded with the cycle
Property the netted stereochemical structure cobalt acid nickel of 3D carbon fiber), make cobalt acid nanosized nickel rods grown on carbon fibers for rule periodicity 3D
Network structure, noble metal nano particles are then coated on the above-mentioned carbon for being loaded with cobalt acid nanosized nickel rods using magnetron sputtering technique
Fiber surface, obtain the SERS substrates of the carried noble metal nano-cluster with 3D reticulated structures.
The detailed process of the hydro-thermal reaction method is：Carbon fiber is divided in acetone, absolute ethyl alcohol and deionized water successively
Other supersound washing 20-30min, it is subsequently placed in 60 DEG C of vacuum drying chambers and dries 12h；It is anti-that dried carbon fiber is placed in high pressure
Answer in kettle, by cobalt salt, nickel salt and ammonium fluoride in molar ratio 1：2：6 be dissolved in deionized water after inject in above-mentioned autoclave, in
100 DEG C of reaction 12h, after reaction terminates, naturally cool to room temperature, take out carbon fiber, rushed repeatedly with absolute ethyl alcohol and deionized water
Wash, be finally placed in 60 DEG C of vacuum drying chambers and dry 12h, produce the carbon fiber for being loaded with cobalt acid nanosized nickel rods.
The magnetron sputtering technique is specially：The carbon fiber for being loaded with cobalt acid nanosized nickel rods is placed in rf magnetron sputtering system
In system, it is 0.1-0.9Pa to control sputtering operating pressure, sputtering power 20-150W, and sputtering rate isDuring sputtering
Between be 10-120s, sputtering thickness is 10-200nm, rotational velocity 5-20rpm, is received by sputtering noble metal to carbon fiber surface
Rice grain, obtain the SERS substrates of the carried noble metal nano-cluster with 3D reticulated structures.
The noble metal being related in the present invention includes the metal good conductors such as gold, silver or copper.The grain of the noble metal nano particles
Footpath is 20-150nm.
The schematic diagram of preparation method of the present invention is shown in Fig. 1.
The present invention also provides the SERS of the carried noble metal nano-cluster with 3D reticulated structures prepared using the above method
Substrate.
Compared with prior art, the advantage of the invention is that：
(1) the netted stereochemical structure cobalt acid nickel of periodicity 3D being prepared using hydro-thermal reaction method is by cobalt acid nickel nanometer
Rod rearranges, and these nanometer rods have a large amount of flat surfaces, is advantageous to the noble metal nano particles of subsequent coated in shape thereon
Into the uniform cluster structure with nanoscale spacing.Meanwhile these superfine cobalt acid nanosized nickel rods have nano level point
End structure, noble metal nano particles thereon can be made further to reunite, be formed and significantly increased in the presence of external exciting light
Electromagnetic field.In addition, the periodic structure of cobalt acid nickel causes the SERS active sites in substrate to be uniformly distributed, this new SERS
Substrate can send the SERS signal of uniformity.
(2) during magnetron sputtering noble metal nano particles, by changing the power sputtered, speed, time, thickness
Degree and rotational velocity etc. can efficiently control the coated weight of noble metal nano particles, so as to efficiently control follow-up SERS
The intensity of signal, a variety of substrates with different SERS signal intensity are obtained, realize highly sensitive controllable detection.In addition, magnetic
Sputtering method green high-efficient is controlled, avoids using substantial amounts of surfactant in the chemical preparation of traditional noble metal nano particles and goes back
The shortcomings that former agent etc. easily pollutes to environment.
(3) preparation technology of the present invention is simple, cost is low, takes less, yield height, easy to spread and large-scale production, due to
The carrier of the SERS substrates is carbon fiber (charcoal cloth), and therefore, the SERS substrates of preparation are flexible, can cut, portable, just
Detected in applied to clinical biochemical medical science, particularly suitable for fields such as high-sensitivity biological chemical sensors.
Brief description of the drawings
Fig. 1 is the principle of the preparation method of the SERS substrates for the carried noble metal nano-cluster that the present invention has 3D reticulated structures
Figure；Wherein, CFC is carbon fiber.
Fig. 2 is the SERS substrates electricity of the load gold nano cluster with 3D reticulated structures prepared in the embodiment of the present invention 1
Sub- microphotograph.
Fig. 3 is the SERS bases using the load gold nano cluster with 3D reticulated structures prepared in the embodiment of the present invention 1
Bottom carries out the result of Raman signal detection to Raman labels molecule 4-MBA.
Fig. 4 is that the SERS substrates for loading ag nano-cluster with 3D reticulated structures prepared in the embodiment of the present invention 2 are electric
Sub- microphotograph.
Fig. 5 is the SERS bases using the load ag nano-cluster with 3D reticulated structures prepared in the embodiment of the present invention 2
Bottom carries out the result of Raman signal detection to Raman labels molecule 4-MBA.
Fig. 6 is the SERS substrates electricity of the supported copper nanocluster with 3D reticulated structures prepared in the embodiment of the present invention 3
Sub- microphotograph.
Fig. 7 is the SERS bases using the supported copper nanocluster with 3D reticulated structures prepared in the embodiment of the present invention 3
Bottom carries out the result of Raman signal detection to Raman labels molecule 4-MBA.
Embodiment
Following examples are used to illustrate the present invention, but are not limited to the scope of the present invention.Unless otherwise specified, embodiment
In the conventional meanses that are well known to those skilled in the art of used technological means, raw materials used is commercial goods.Charcoal cloth (carbon
Fiber) it is commercially available prod, model 3K.Raman spectrum detector BWS415 is purchased from Bi Da Imtech of the U.S. (B＆W Tek
Inc.)。
Embodiment 1 has the preparation of the SERS substrates of the load gold nano cluster of 3D reticulated structures
The preparation method of the SERS substrates of load gold nano cluster with 3D reticulated structures comprises the following steps：
The carbon fiber that cobalt acid nanosized nickel rods are loaded with using the preparation of hydro-thermal reaction method (is loaded with the netted solids of periodicity 3D
The flexible charcoal cloth of structure cobalt acid nickel), make periodicity 3D network structure of the cobalt acid nanosized nickel rods in grown on carbon fibers for rule.Tool
Body process is：Carbon fiber is distinguished into supersound washing 20-30min in acetone, absolute ethyl alcohol and deionized water successively, is subsequently placed in
12h is dried in 60 DEG C of vacuum drying chambers；Dried carbon fiber is placed in autoclave, by cobalt salt, nickel salt and ammonium fluoride
In molar ratio 1：2：6 be dissolved in deionized water after inject in above-mentioned autoclave, in 100 DEG C react 12h, reaction terminate after, from
Room temperature is so cooled to, carbon fiber is taken out, is rinsed, be finally placed in 60 DEG C of vacuum drying chambers repeatedly with absolute ethyl alcohol and deionized water
12h is dried, produces the carbon fiber for being loaded with cobalt acid nanosized nickel rods.
The above-mentioned carbon fiber for being loaded with cobalt acid nanosized nickel rods is placed in rf magnetron sputtering system, control sputtering work pressure
Power is 0.3Pa, sputtering power 50W, and sputtering rate isSputtering time is 50s, and sputtering thickness is 30nm, from rotating speed
Spend for 10rpm, pass through to carbon fiber surface and sputter the gold nano grain that particle diameter is 80nm, obtain the load with 3D reticulated structures
The SERS substrates of gold nano cluster.
Fig. 2 shows the SERS substrate electronics of the load gold nano cluster with 3D reticulated structures prepared in the present embodiment
Microphotograph, figure it is seen that prepared gold nano grain forms substantial amounts of group at the surface of cobalt acid nickel and tip
Clustering architecture, and the spacing of these clusters is nanoscale.
Fig. 3 is the SERS substrates pair for the load gold nano cluster with 3D reticulated structures being prepared using the above method
Raman labels molecule 4- mercaptobenzoic acids (4-MBA) carry out Raman signal detection, obtained Raman spectrogram.4- used during detection
The concentration of MBA solution is 4 × 10-8M, the power of laser used is 30mW, time of integration 10s.From figure 3, it can be seen that should
SERS active-substrate has good SERS signal enhancement effect, and it is in 1078cm-1The Raman signal intensity at place is up to 25000.
Embodiment 2 has the preparation of the SERS substrates of the load ag nano-cluster of 3D reticulated structures
The preparation method of the SERS substrates of load ag nano-cluster with 3D reticulated structures comprises the following steps：
The carbon fiber that cobalt acid nanosized nickel rods are loaded with using the preparation of hydro-thermal reaction method (is loaded with the netted solids of periodicity 3D
The carbon fiber of structure cobalt acid nickel), make periodicity 3D network structure of the cobalt acid nanosized nickel rods in grown on carbon fibers for rule, the party
Description of the method with embodiment 1.
The above-mentioned carbon fiber for being loaded with cobalt acid nanosized nickel rods is placed in rf magnetron sputtering system, control sputtering work pressure
Power is 0.6Pa, sputtering power 80W, and sputtering rate isSputtering time is 80s, and sputtering thickness is 50nm, from rotating speed
Spend for 15rpm, pass through to carbon fiber surface and sputter the silver nano-grain that particle diameter is 150nm, obtain negative with 3D reticulated structures
The SERS substrates of silver-carrying nano cluster.
Fig. 4 shows that what is prepared in the present embodiment has the SERS substrate electronics of the load ag nano-cluster of 3D reticulated structures
Microphotograph, from fig. 4, it can be seen that prepared silver nano-grain forms substantial amounts of group at the surface of cobalt acid nickel and tip
Clustering architecture, and the spacing of these clusters is nanoscale.
Fig. 5 is the SERS substrates pair for the load ag nano-cluster with 3D reticulated structures being prepared using the above method
Raman labels molecule 4- mercaptobenzoic acids (4-MBA) carry out Raman signal detection, obtained Raman spectrogram.4- used during detection
The concentration of MBA solution is 4 × 10-8M, the power of laser used is 30mW, time of integration 10s.From fig. 5, it can be seen that should
SERS active-substrate has good SERS signal enhancement effect, and it is in 1078cm-1The Raman signal intensity at place is up to 30000.
Embodiment 3 has the preparation of the SERS substrates of the supported copper nanocluster of 3D reticulated structures
The preparation method of the SERS substrates of supported copper nanocluster with 3D reticulated structures comprises the following steps：
The carbon fiber that cobalt acid nanosized nickel rods are loaded with using the preparation of hydro-thermal reaction method (is loaded with the netted solids of periodicity 3D
The carbon fiber of structure cobalt acid nickel), make periodicity 3D network structure of the cobalt acid nanosized nickel rods in grown on carbon fibers for rule, the party
Description of the method with embodiment 1.
The above-mentioned carbon fiber for being loaded with cobalt acid nanosized nickel rods is placed in rf magnetron sputtering system, control sputtering work pressure
Power is 0.8Pa, sputtering power 100W, and sputtering rate isSputtering time is 100s, and sputtering thickness is 180nm, from
Rotary speed is 18rpm, by sputtering the copper nano particles that particle diameter is 20nm to carbon fiber surface, is obtained with 3D reticulated structures
The SERS substrates of supported copper nanocluster.
Fig. 6 shows the SERS substrate electronics of the supported copper nanocluster with 3D reticulated structures prepared in the present embodiment
Microphotograph, from fig. 6, it can be seen that prepared copper nano particles form substantial amounts of group at the surface of cobalt acid nickel and tip
Clustering architecture, and the spacing of these clusters is nanoscale.
Fig. 7 is the SERS substrates pair for the supported copper nanocluster with 3D reticulated structures being prepared using the above method
Raman labels molecule 4- mercaptobenzoic acids (4-MBA) carry out Raman signal detection, obtained Raman spectrogram.4- used during detection
The concentration of MBA solution is 4 × 10-8M, the power of laser used is 30mW, time of integration 10s.From figure 7 it can be seen that should
SERS active-substrate has good SERS signal enhancement effect, and it is in 1078cm-1The Raman signal intensity at place is up to 20000.
Although above the present invention is described in detail with a general description of the specific embodiments,
On the basis of the present invention, it can be made some modifications or improvements, this will be apparent to those skilled in the art.Cause
This, these modifications or improvements, belong to the scope of protection of present invention without departing from theon the basis of the spirit of the present invention.
Claims (7)
1. the preparation method of the SERS substrates of the carried noble metal nano-cluster with 3D reticulated structures, it is characterised in that utilize water
Thermal response method prepares the carbon fiber for being loaded with cobalt acid nanosized nickel rods, makes week of the cobalt acid nanosized nickel rods in grown on carbon fibers for rule
Phase property 3D network structures, noble metal nano particles are then loaded with cobalt acid nickel nanometer coated on above-mentioned using magnetron sputtering technique
The carbon fiber surface of rod, obtain the SERS substrates of the carried noble metal nano-cluster with 3D reticulated structures.
2. preparation method according to claim 1, it is characterised in that the detailed process of the hydro-thermal reaction method is：By carbon
Fiber distinguishes supersound washing 20-30min in acetone, absolute ethyl alcohol and deionized water successively, is subsequently placed in 60 DEG C of vacuum drying
12h is dried in case；Dried carbon fiber is placed in autoclave, by cobalt salt, nickel salt and ammonium fluoride in molar ratio 1：2：6
Injected after being dissolved in deionized water in above-mentioned autoclave, 12h reacted in 100 DEG C, after reaction terminates, naturally cools to room temperature,
Carbon fiber is taken out, is rinsed repeatedly with absolute ethyl alcohol and deionized water, is finally placed in 60 DEG C of vacuum drying chambers and dries 12h, produce
It is loaded with the carbon fiber of cobalt acid nanosized nickel rods.
3. preparation method according to claim 1, it is characterised in that the magnetron sputtering technique is specially：It will be loaded with
The carbon fiber of cobalt acid nanosized nickel rods is placed in rf magnetron sputtering system, and it is 0.1-0.9Pa to control sputtering operating pressure, sputters work(
Rate is 20-150W, and sputtering rate isSputtering time is 10-120s, sputters thickness 10-200nm, and rotational velocity is
5-20rpm, by sputtering noble metal nano particles to carbon fiber surface, obtain the carried noble metal nanometer with 3D reticulated structures
The SERS substrates of cluster.
4. according to the preparation method described in claim any one of 1-3, it is characterised in that the noble metal includes gold, silver or copper.
5. preparation method according to claim 4, it is characterised in that the particle diameter of the noble metal nano particles is 20-
150nm。
6. the carried noble metal nanometer with 3D reticulated structures prepared according to method any one of claim 1-3 or 5
The SERS substrates of cluster.
7. the SERS substrates of the carried noble metal nano-cluster with 3D reticulated structures prepared by method according to claim 4.
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| CN113324970B (en) * | 2021-04-25 | 2023-04-21 | 中国科学技术大学 | Structure-adjustable high-hot-spot three-dimensional mesh screen nano Raman substrate and preparation and application thereof |
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